ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Hydrochloric Acid → 4,5-difluoro-2-[[3-methyl-1-(6-methyl-2-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid

HRID 498071
ノート
印刷プレビュー

反応式

HRID 498071 の反応式
[CH3:1][C:2]1[CH:6]=[C:5]([NH2:7])[N:4]([C:8]2[CH:13]=[CH:12][CH:11]=[C:10]([CH3:14])[N:9]=2)[N:3]=1.Cl[C:16]1[CH:24]=[C:23]([F:25])[C:22]([F:26])=[CH:21][C:17]=1[C:18]([OH:20])=[O:19].C(=O)([O-])[O-].[K+].[K+].Cl>CN(C)C=O.C([O-])(=O)C.[Cu+2].C([O-])(=O)C.O>[F:25][C:23]1[C:22]([F:26])=[CH:21][C:17]([C:18]([OH:20])=[O:19])=[C:16]([NH:7][C:5]2[N:4]([C:8]3[CH:13]=[CH:12][CH:11]=[C:10]([CH3:14])[N:9]=3)[N:3]=[C:2]([CH3:1])[CH:6]=2)[CH:24]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

8

反応物 4

HCID 313Hydrochloric AcidHCID 11430Potassium CarbonateHCID 7371712-Chloro-4,5-difluorobenzoic acidHCID 574177003-Methyl-1-(6-methyl-2-pyridinyl)-1H-pyrazol-5-ylamine

生成物 1

HCID 223203564,5-difluoro-2-[[3-methyl-1-(6-methyl-2-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid収率 79.2%

試薬・触媒・溶媒 3

HCID 8895
Cupric acetate
触媒
HCID 962Water溶媒
HCID 6228Dimethylformamide溶媒

実験手順

A solution of 3-methyl-1-(6-methyl-2-pyridinyl)-1H-pyrazol-5-ylamine (5.65 g, 30.0 mmol), 2-chloro-4,5-difluorobenzoic acid (6.93 g, 36.0 mmol), copper acetate (II) (0.545 g, 3.00 mmol) and potassium carbonate (4.15 g, 30.0 mmol) in N,N-dimethylformamide (30 mL) was heated under reflux under an argon atmosphere for 2 hours. The solution was allowed to cool to room temperature, and the reaction mixture was poured into water. The solution was made weakly acidic by the addition of 1N hydrochloric acid, and the resulting crude crystals were collected by filtration. The crystals were washed with water and air dried to give crude 4,5-difluoro-2-[[3-methyl-1-(6-methyl-2-pyridinyl)-1H-pyrazol-5-yl]amino]benzoic acid (8.18 g, 79% yield). A solution of the compound (7.00 g, 20.3 mmol) in phosphorus oxychloride (9.73 mL, 104 mmol) was heated under reflux for 30 minutes. The reaction solution was allowed to cool to room temperature, and the residue was poured into iced water. The solution was neutralized by the addition of a sodium hydroxide solution, and the organic matter was extracted with chloroform. The extract was washed with saturated brine and water, dried over anhydrous magnesium sulfate, and the solvent was evaporated under reduced pressure. The residue thus obtained was purified by silica gel column chromatography (chloroform) to give crude 4-chloro-6,7-difluoro-3-methyl-1-(6-methyl-2-pyridinyl)-1H-pyrazolo[3,4-b]quinoline (2.70 g, 39% yield). To a solution of the compound (2.70 g, 36.0 mmol) in ethanol (120 mL), 6N hydrochloric acid (4 mL, 24.0 mmol) was added, and the mixture was heated under reflux for 3 hours. The reaction solution was allowed to cool to room temperature, and the resulting crystals were collected by filtration. The crystals were washed with ethanol, air dried and recrystallized from ethanol to give the title compound (1.68 g, 66% yield).

後処理

  1. temperatureunder reflux under an argon atmosphere for 2 hours
  2. filtrationthe resulting crude crystals were collected by filtration
  3. washThe crystals were washed with water and air
  4. customdried

出典と根拠

ORDレコード
ord-6db02f72bb794b4bbb11b182d4d62207
出典データセット
uspto-grants-2005_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06949648B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート